Methyl Anthranilate → Methyl 2-[(4-ethoxy-4-oxobutyl)amino]benzoate

HRID 1457646ノート

反応式

HRID 1457646 の反応式
[NH2:1][C:2]1[CH:11]=[CH:10][CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5].Br[CH2:13][CH2:14][CH2:15][C:16]([O:18][CH2:19][CH3:20])=[O:17]>>[CH3:7][O:6][C:4](=[O:5])[C:3]1[CH:8]=[CH:9][CH:10]=[CH:11][C:2]=1[NH:1][CH2:13][CH2:14][CH2:15][C:16](=[O:17])[O:18][CH2:19][CH3:20]

参加物

3

反応物 2

HCID 8635Methyl AnthranilateHCID 76300Ethyl 4-bromobutyrate

生成物 1

HCID 266836Methyl 2-[(4-ethoxy-4-oxobutyl)amino]benzoate

実験手順

A mixture of 19.2 g of methyl 2-aminobenzoate and 9.6 g of ethyl γ-bromobutyrate is heated at 80°-85° C. for 24 hours, cooled to room temperature and filtered. The solid is washed with CH2Cl2 and the filtrate washed with 1NHCl, H2O, 1NNaHCO3 and brine. The solvent is removed to give an oil. The oil is distilled and the fraction boiling at 45°-75° C. and 130°-160° C. were collected and discarded. The residue is the product (55.4 g of oil)

後処理

  1. temperatureis heated at 80°-85° C. for 24 hours
  2. filtrationfiltered
  3. washThe solid is washed with CH2Cl2
  4. washthe filtrate washed with 1NHCl, H2O, 1NNaHCO3 and brine
  5. customThe solvent is removed
  6. customto give an oil
  7. distillationThe oil is distilled
  8. customthe fraction boiling at 45°-75° C. and 130°-160° C. were collected

出典と根拠

ORDレコード
ord-d62bb3baf13843af8b33c6b88aed4eaa
出典データセット
uspto-grants-1998_12
特許番号
US05849735

反応ノート

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